• Title/Summary/Keyword: GC/MS spectrometry

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Monitoring of Benzoic, Sorbic and Propionic Acid in Cereal Grains, Nuts and Seeds (곡류 및 견과 종실류 중 안식향산, 소브산, 프로피온산의 함유량 조사)

  • Yun, Sang Soon;Lee, Sang Jin;Lim, Do Yeon;Lim, Ho Soo;Lee, Gunyoung;Kim, MeeKyung
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.65-72
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    • 2019
  • This study was aimed at investigating the levels of the natural preservatives of benzoic, sorbic and propionic acids in cereal grains, nuts and seeds. Benzoic and sorbic acid were analyzed by high-performance liquid chromatography with a diode-array detector (HPLC-DAD) and further confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), whereas propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and further confirmed by gas chromatography-mass spectrometry (GC-MS). Benzoic, sorbic and propionic acids were found in 44, 22, and 550 samples out of 702 samples, respectively. From the total of 702 samples. The concentrations of benzoic, sorbic and propionic acid were ranged from not detected (ND) to 23.74 mg/L, from ND to 7.90 mg/L, and from ND to 37.39 mg/L in cereal grains, nuts and seeds, respectively. The concentration ranges determined in this study could be used as standard criteria in the process of inspecting cereal grains, nuts and seeds for preservatives as well as to address consumer complaints or trade disputes.

Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

Studies on the Volatile Aroma Components of Pleurotus ostreatus (느타리버섯의 향기(香氣) 성분(成分)에 관한 연구(硏究))

  • Hong, Jai-Sik;Lee, Ji-Yul;Kim, Young-Hoi;Kim, Myung-Kon;Jung, Gi-Tae;Lee, Keug-Ro
    • The Korean Journal of Mycology
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    • v.14 no.1
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    • pp.31-36
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    • 1986
  • The volatile aroma concentrates were isolated from Pleurotus ostreatus by simultaneous distillation-extraction and analyzed by gas chromatography and combined gas chromatography-mass spectrometry. The aroma concentrates obtained had a typical raw or slightly cooked mushroom-like odor, and the yield was 123 ppm. Of 27 components identified, the major components were 3-octanone, 3-octanol, 2-octenal, n-octanol and 2, 4-decadienal, including 1-octen-3-ol contributing 67.06% of the total volatiles, and the $C_8$ compounds comprised about 80% of the total volatiles. On the other hand, the $C_6$ and $C_8$ alcohols in mushroom increased gradually with increase of standing time after homogenation, while aldehydes, ketones, and linoleic acid decreased, and also $C_6$ and $C_8$ compounds were significantly increased when linoleic and linolenic acid were added in homogenates. It appears that most of volatile aroma components in Pleurotus ostreatus were probably produced enzymatically from unsaturated fatty acids containing cis, cis-1, 4-pentadiene moiety.

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Analysis of Environmental Odor Factors for Dorim Stream in Gwanak-gu, Seoul (서울시 관악구 도림천 복개 정도에 따른 환경 악취 요인 분석)

  • Soyoung Park;Gokce Nur Ayaz;Heewon Kim;Hyungkee Yoon;Taehong Kwon;Sungkyoon Kim
    • Journal of Environmental Health Sciences
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    • v.50 no.2
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    • pp.83-92
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    • 2024
  • Background: In this study, we investigate the rapid increase in environmental odors and notable rise in civil complaints near Dorim Stream in the Gwanak-gu area of Seoul. Objectives: This study aims to identify the causal compounds responsible for environmental odors in the Dorim Stream and investigate the structural characteristics of the stream that influence odor generation. Methods: The research methodology involved setting up 41 sampling points, selecting panels for direct sensory evaluation to assess odor intensity, measuring dissolved oxygen and hydrogen sulfide concentrations, and using all-in-one low-temperature desorption gas chromatography (ATD-GC) and thermal desorption-gas chromatography-mass spectrometry (TD-GC/MS) analysis to identify odor-causing compounds. Results: The evaluation of Dorim Stream revealed that in areas with complete meandering, there were lower dissolved oxygen levels (4.5±2.67 mg/L) and higher odor intensity (4.0±0.92), while in partially meandering sections, higher dissolved oxygen levels (7.8±1.15 mg/L) and lower odor intensity (2.8±1.06) were observed. Hydrogen sulfide levels measured with sensors increased with higher temperatures, especially in the afternoon hours (12:00~14:00). Acetaldehyde was the dominant odor compound detected in both the Bonglim Bridge (0.4 ppm) area and Guro Bridge area (0.867 ppm), with concentrations more than twice as high near Guro Bridge. Odor-causing compounds identified by TD-GC/MS indicated a pungent, sulfurous odor in the Guro Bridge area and a musty odor in the Bonglim Bridge area. Conclusions: This study categorizes and analyzes the sources of odor in Dorim Stream in Seoul based on meandering patterns and the distribution of sewage facilities, highlighting the potential odor issues associated with combined sewage systems and sewer junctions and suggesting policy improvements.

Development of Analytical Method for the Determination and Identification of Unregistered Pesticides in Domestic for Orange and Brown Rice(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide- (식품공전 분석법 미설정 농약의 잔류분석법 확립(I) -Chlorthal-dimethyl, Clomeprop, Diflufenican, Hexachlorobenzene, Picolinafen, Propyzamide-)

  • Chang, Hee-Ra;Kang, Hae-Rim;Kim, Jong-Hwan;Do, Jung-A;Oh, Jae-Ho;Kwon, Ki-Sung;Im, Moo-Hyeog;Kim, Kyun
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.157-163
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    • 2012
  • BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.

Rancidity Analysis of Rapeseed Oil under Different Storage Conditions Using Mass Spectrometry-based Electronic Nose (질량분석기 기반-전자코를 이용한 저장중 유채유의 산패 분석)

  • Hong, Eun-Jeung;Lim, Chae-Lan;Son, Hee-Jin;Choi, Jin-Young;Noh, Bong-Soo
    • Korean Journal of Food Science and Technology
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    • v.42 no.6
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    • pp.699-704
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    • 2010
  • Rapeseed oil was stored under different conditions such as in the dark, with UV treatment, and with prooxidantscytochrome C and copper ion. The rapeseed oils stored at different temperatures were analyzed by a mass spectrometrybased electronic nose and discriminant function analysis (DFA). Volatile components in the rapeseed oil increased with storage time, and the discriminant function first score (DF1) moved from a positive position to a negative position as storage time increased. Changes in DF1 were higher under UV treatment than under the dark condition (DF1: $r^2$=0.9481, F=307.03). The different DF1 values (F1) under the dark condition were 0.099, 0.187, and 0.278 as storage temperature increased. The different values under UV treatment were 0.554, 0.588, and 0.542, as storage temperature increased from 4 to $26^{\circ}C$. As concentrations of prooxidants copper ion and cytochrome C increased, amounts of volatile components also increased. These were confirmed by DFA. Furthermore, changes in responses at each ion fragment agreed with reported results for GC/MS, which formed after rancidity of the oil, including pentane, pentanal, 1-pentanol, hexanal, n-octane, 2-hexenal, heptanal, 2-heptenal, decane, 2-octenal, undecane, and dodecane.

Preserving Reliability of Evidence Containers for Fire Debris Containing Ignitable Liquids (유류화재증거물 보관용기의 신뢰성에 관한 연구)

  • Han, Dong-Hun;Lee, Sung-Ryong
    • Fire Science and Engineering
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    • v.27 no.2
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    • pp.70-74
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    • 2013
  • It is very important for the collected samples at fire scenes to be properly preserved for laboratory analysis. Preserving abilities of four type containers, metal cans, glass jars, zipper and heat sealed polymer bags, with the five ignitable liquids (toluene, n-octane, o-xylene, n-decane and n-hexadecane) were examined with gas chromatography-mass spectrometry. The glass jars with Teflon (PTFE) liner were the best ability to prevent the evaporation of the ignitable liquids.

Seasonal Variation in Concentration and Composition of Monoterpenes from Artemisia princeps var. orientalis (쑥에 함유된 monoterpenes 의 함량과 조성의 계절적 변이)

  • Kim, Jong-Hee
    • The Korean Journal of Ecology
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    • v.19 no.4
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    • pp.321-328
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    • 1996
  • The profile and concentration of monoterpene metabolites in the leaf and stem of Artemisia princeps var. orientalis were quantified, and seasonal variation in monoterpenes of Artemisia plant was investigated. Samples were taken from five sites at the campus of Kyungnam University during maturing season. Monoterpenes in leaf and stem were analyzed using gas chromatography-mass spectrometry (GC-MS). The major constituents of A. princeps var. orientalis in both the leaf and stem were 21 monoterpenes.$ {\alpha}-pinene,\;{\beta}-pinene,\;{\beta}-myrcene$, dl-limonene, naphthalene and unknown monoterpenes with 5.49 and 16.27 of retenstion time were present in high concentrations of compounds identified on the leaf and stem of A. princeps var. orientalis. The cmounts of total monoterpenes of leaf were from two to five times higher than stem and rapidly decreased with the time, while that of stem was constnat except early spring. Most of the high percentage of monoterpenes in the leaf were those with later retention time. These results indicated that monoterpenes yields are considered to be more variable than monoterpene composition in responding to the time in both the leaf and stem.

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Determination of Phthalates in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 프탈산 에스텔류의 분석법)

  • Seo, Jung-Ju;Na, Yuncheol;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.400-409
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    • 2001
  • A method for the analysis of most common phthalate acid esters (9 secies) in biota samples by gas chromatography-mass spectrometry-selected ion monitoring mode is described. Phthalates in biota samples are extracted by organic solvent and purified by Florisil column. Phthalates are easily contaminated during extraction prodedure. Since the extraction and cleanup steps for biota samples generally are more complicate than those for water or sediment samples, we compared with contamination state of each sample work-up step. By applying this developed method, the overall recoveries ranged between 79 - 117% in biota sample which was spiked with standards. For phthalates used in this study, the quantitaive accuracy, elution pattern on Florisil column, and detection limits were also investigated.

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Determination of 4-Nitrotoluene Exposure in Water, Soil and Sediment by Gas Chromatography- Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 토양, 저질 및 수질시료 중 4-Nitrotoluene의 노출평가)

  • Jeon Hee Kyung;Choi Hae Yeon;Ryu Jae-Chun
    • Environmental Analysis Health and Toxicology
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    • v.20 no.2 s.49
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    • pp.123-131
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    • 2005
  • 본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 4-Nitrotoluene(4-NT)을 분석하는 방법을 확립하고자 하였다. 4-NT은 수질 시료(100mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료(10g)에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 4-NT의 회수율은 $99.1\%$ 이상이였으며 토양에서의 회수율(recovery)은 약 $110\%$를 보였고 재현성 (relative standard deviation)은 $11.99\%$ 이하였다. 검정곡선은 상관계수$(R^2)$값이 수질과 토양 모두에서 0.994이상의 좋은 직선성을 보여주었다. 본 연구에서 채취한 수질 43개 지역, 토양 35개 지역 및 저질 11개 지역의 모든 시료에서 4-NT은 검출한계 이하로 나타났다. 이 분석방법은 환경 중에 미량으로 존재하는 4-NT의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.